EP3872477B1 - Systeme et procede pour la mesure de carburants fluides - Google Patents

Systeme et procede pour la mesure de carburants fluides Download PDF

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Publication number
EP3872477B1
EP3872477B1 EP21159799.2A EP21159799A EP3872477B1 EP 3872477 B1 EP3872477 B1 EP 3872477B1 EP 21159799 A EP21159799 A EP 21159799A EP 3872477 B1 EP3872477 B1 EP 3872477B1
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EP
European Patent Office
Prior art keywords
measurement
valve
sensor unit
chamber
pump
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EP21159799.2A
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German (de)
English (en)
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EP3872477C0 (fr
EP3872477A1 (fr
Inventor
Wojciech Knap
Tomasz Skotnicki
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Instytut Wysokich Cisnien of PAN
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Instytut Wysokich Cisnien of PAN
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
    • G01N21/3581—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light using far infrared light; using Terahertz radiation
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
    • G01N21/3577—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing liquids, e.g. polluted water
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/26—Oils; Viscous liquids; Paints; Inks
    • G01N33/28—Oils, i.e. hydrocarbon liquids

Definitions

  • the invention concerns a measurement system and a measurement method of fluid fuels, in particular liquid, and in particular gasoline, by means of spectrometers.
  • Fluid fuels, in particular gasoline are easily degenerated.
  • solutions on the base of spectrum analysis allowing for a quality assessment and a degeneration detection are known.
  • CN102323235A a quality assessment by means of spectrum analysis by spectrums comparison is disclosed.
  • the spectrometer is enclosed in a vacuum chamber with pumps and a gas port.
  • the pressure is monitored using a vacuum gauge. Gases are flowed continuously through the chamber, and the pressure is controllable in increments of about 1-5 mTorr using a single needle valve.
  • JOURNAL OF PHYSICS D APPLIED PHYSICS, INSTITUTE OF PHYSICS PUBLISHING LTD, GB, vol. 49, no. 39, 6 September 2016 (2016-09-06)
  • page 395101 a spectral analysis of fuel oils using terahertz radiation is disclosed.
  • a THz- time domain conventional spectroscopy system with single spectrometer is disclosed.
  • Drawbacks of spectrum analysis include its sensitivity to measurement conditions - in particular pressure. It is troublesome when measuring gaseous fuels, in particular under conditions of carrying out measurements in gas pipelines.
  • Drawbacks of spectrum analysis of liquids include impossibility of identification of components due to diffusion of characteristic spectrums for particular components.
  • the measurement system of fluid fuels according to the invention is defined in claim 1. Thanks to such configuration, by means of the terahertz and subterahertz spectrometer, it is possible to carry out accurate measurements of spectrometry of gas collected to the measurement chamber or gas obtained from evaporation of liquid fuel, simultaneously ensuring stable measurement conditions independent from state of gas in the line and optimized for the sensitivity.
  • the result can be compared to a reference absorption spectrum measured by other methods and a warning message can be displayed, if a discrepancy between measurement and the reference spectrum meets a predefined criterion.
  • the measurement can be at carried out by opening the first valve releasing fuel vapours, then the measurements are carried out with the spectrometers and a result is recorded, whereupon the second valve is opened and by means of the pump, fuel vapours are pumped out from the chamber of the sensor unit.
  • Dynamic flow is constituted by fuel vapours, which change from liquid to gaseous state upon exposure of small amount of fluid transferring via the valve in the chamber of the sensor unit to the state close to vacuum.
  • two spectrometers are used, by means of which the measurement is carried out sequentially.
  • At least one spectrometer constitutes the semiconductor subterahertz spectrometer, with an operating band falling within the range of 100 GHz to 1000 GHz and the measurement by means of this spectrometer is carried out as the last.
  • Fig. 1a shows a block diagram of a measurement system of fluid fuels according to an embodiment of the invention
  • Fig. 1b shows a block diagram of a measurement system of fluid fuels according to an alternative embodiment the invention
  • Fig. 2 schematically shows a measuring chamber with spectrometers in a sensor unit according to an embodiment of the invention (a control unit has not been shown in Fig. 2 ).
  • FIG. 1a A block diagram of the measurement system of fluid fuels in the embodiment of the invention was shown in Fig. 1a .
  • the system is suitable to be mounted on a line R1 carrying fluid fuel, in particular gasoline.
  • a branching unit T1 is provided, discharging a part of fluid fuel and secured with the first valve V1 constituting a needle valve. Partial opening of the first needle valve V1 allows for introducing into the sensor unit K1 comprising a measurement chamber with a spectrometer, gaseous fuel or liquid fuel vapours, which are subject to a spectroscopic analysis. Good effects were achieved by using a semiconductor subterahertz spectrometer with an operating band falling within the range of 100 GHz to 1000 GHz.
  • the sensor unit K1 is placed between two valves, the first valve V1 and the second valve V2, thanks to which the measurement can be carried out under conditions set at the particular moment.
  • a manometer M1 is used for measuring pressure in the measuring chamber.
  • the needle valve with a control unit of the valve B1 connected to the manometer M1 was used for measuring pressure in the measuring chamber. Thanks to this it is possible to measure out the proper pressure from the line R1, specific for the measurement, regardless prevailing conditions in the line R1: pressure and flow rate. Thanks to this, by measuring out gas by the first valve V1, a result of the measurement is independent from pressure changes in the line R1.
  • Using the additional pump P1 allows for precise pressure regulation in the chamber of the sensor unit K1.
  • Terahertz spectrometers showed higher sensitivity and the ability to distinguish wider spectrum of contaminant substances, although the measurement by means of them lasts longer.
  • the sensor unit K1 is connected to the control unit C1 generating a control signal for the sensor unit K1 and receiving the measurement result.
  • a knowledge of a reference spectrum and an adoption of a discrepancy criterion in the way known in the state-of-the-art allows for generating a message generation by a display W1 connected to the control unit C1.
  • the control unit C1 can be also used to control the pump P1 and the first valve V1 and the second valve V2.
  • a coupling of the first valve with the manometer M1 - via the control unit of the valve B1 and/or via the control unit C1 allows for dosing fuel subjected to the measurement by means of using the pump P1, what allows for repeating the measurement in pressure conditions significantly below atmospheric pressure.
  • it can be provided a unit cutting off fuel supply in the case of detection of a contaminant dangerous for a receiver. For this, it is sufficient to provide a controllable valve connected to the control unit C1.
  • Feeding the signal from the manometer M1 to the control unit C1 allows for inclusion of pressure in determining the measurement result as well as carrying out the measurement for different pressure values.
  • the measurement system according to the invention can also be used for measuring fluid fuel in a container. Such configuration is shown on Fig. 1b . Fuel from a container Z1 is collected by means of the branching unit T1. A coupling of the first valve with the manometer M1 via a control unit C1 allows for measuring fuel subjected to the measurement by means of the pump P1, what allows for repeating the measurement in conditions significantly below atmospheric pressure - in dynamic pressure conditions. In the case of fluid fuels it is so advantageous, that liquid fuel exposed to vacuum evaporates forming dynamic flow allowing for accurate and continuous measurement without broadening of spectral lines characteristic for liquids.
  • Described herein are the modes of operation of the system: it can operate in a continuous mode or in a sequential mode.
  • the system operates in a cycle, in which in the chamber of the sensor unit K1 secured from the both sides by the first valve V1 and second valve V2, initially there is a vacuum, then the unit is filled with fluid measured by means of the first valve V1 opened for the short time - if necessary, several times - up to achieving proper measuring pressure. Then, the measurement is carried out and a result is recorded, after which the second valve V2 is opened and by means of the pump P1 fluid is pumped out, achieving vacuum in the measuring chamber again. The measurement can be repeated, achieving a sampling effect of measurement in real time.
  • the first needle valve V1 is opened partially, simultaneously enforcing the operation of the pump P1.
  • the range of the opening of the first needle valve V1 and pump thrust is regulated so that in the chamber of the sensor unit K1 arises so called constant vacuum with dynamic flow.
  • Good and stabilized value of dynamic vacuum can be obtained via electronic control of the first needle valve V1 or both valves - the first valve V1 and the second valve V2.
  • Such configuration proved to be particularly advantageous. It can be maintained even via a simple coupling of the first valve V1 with the manometer and simultaneously vacuum state with dynamic flow provides continuous gas exchange and stable state of favourable measurement conditions.
  • Reference spectrums of non-degenerated fluid fuel, in particular gasoline can be obtained by carrying out the measurement of a calibration sample or by using measurements obtained by other methods. In a process of measurement of reference samples with different level of contamination it is easy to match permissible deviations of the spectrum from the reference.
  • the chambers of this type are commonly used in spectroscopy, due to low interference level, weak chemical activity and sorption activity of quartz as well as a possibility of fast and effective cleansing of the chamber during heating and vacuum pumping. In this case, some losses during transfer caused by electromagnetic wave scattering play a beneficial role, reducing an effect of interference related to multiple radiation reflections from walls and ends of the chamber.
  • the terahertz spectrometer can be used for example as the first spectrometer, with the source S1 and the detector D1, placed next to the openings in the chamber windows of the system of the spectrometers and next to the openings in the mirrors L1, using signal mixing and operating in the band falling within the range of 1 THz to 2 THz.
  • An example of this spectrometer is disclosed in the publication C. Hepp, S. Lüttjohann, A. Roggenbuck, A. Deninger, S. Nellen, T. Göbel, M. Jörger1 and R. Harig1 entitled "A cw-Terahertz Gas Analysis System with ppm Detection Limits". Such spectrometers are currently offered by the Toptica company.
  • a photonic spectrometer operating in the time domain can be used, with the source S2 and the detector D2, placed next to the openings in the windows of the chamber of the system of the spectrometers K1 and next to the openings in the mirrors L2.
  • the third spectrometer can be used for example an aforementioned semiconductor subterahertz spectrometer, with the operating band falling within the range of 100 GHz to 1000 GHz.
  • This spectrometer allows for determining of gas concentration and fast analysis of a mixture of gases on the basis of absorption changes and radiation emission by particles included in gas composition.
  • Radiation frequency range analyzing the gas composition is chosen so to cover characteristic absorption lines of contaminants and thus it enables identifying and differentiating those gases in contaminated hydrogen.
  • the analysis can be carried out by using the optical chamber (optical cavity), provided in the chamber of the sensor unit K1 located between mirrors L3. In the chamber controlled conditions are provided: pressure, volume, temperature suitable for absorption analysis and radiation emission. Measurement process is controlled by the control unit C1 (not shown in Fig.
  • Absolute values of the absorption/emission coefficient are not subject to the direct measurement, but instead their changes caused by phase switching and/or radiation frequency - temporary effects. Sensitivity of spectrometers based on the temporary effects is approaching to the theoretical limits and their resolution is limited by the Doppler effect only, which is practically non-existent in the system secured with valves from the both sides - by the first valve V1 and by the second valve V2.
  • a spectrometer with a variable frequency can be used - e.g. disclosed in V. Vaks, E. Domracheva, E. Sobakinskaya, and M. Chernyaeva, "High precise terahertz spectroscopy for noninvasive medicine diagnostics," Photonics & Lasers in Medicine, vol.
  • the sources S1, S2, S3 and the detectors D1, D2, D3 are connected to the control unit C1 and they are operating under its control. The connections are not shown in the figures for simplification.
  • the control unit C1 serves both to trigger the source operation as well as to receive and process measurement results and control operation of the valves.
  • the accuracy during determination of the instantaneous value of frequency of the radiation source shall not exceed 10 -6 .
  • Such accuracy is achieved by means of the arrangement of a phased-locked loop PLL.
  • the control signal of the frequency of the source can be placed on a dedicated reference input.
  • a reference synthesizer with high frequency stability can be used.
  • a 16-bit high speed converter can form a sweeping signal (in order to obtain a shape of control voltage close to triangular) of control frequency sweeping for signal generator submitted to duplication for achieving measuring radiation of the source S3.
  • Module of the detector D3 can comprise a recording camera on the basis of the waveguide detector with a Schottky diode, a low-noise preamplifier with a polarization circuit of the detector and a low-pass filter (LPF).
  • DC direct current
  • the signal from the preamplifier can be sent onto the input of a very fast analog-to-digital converter, and then to a very fast digital memory, in which spectroscopic signals can be summed and averaged. Then, data can be transferred to the control unit C1, where averaging can be continued. Consistent signal collection allows for increasing of the signal-to-noise ratio, and therefore the sensitivity of the spectroscopic measurements.
  • optical and photonic spectrometers including infrared (near infrared and far infrared), and ultraviolet, as well as spectrometers for visible band, can be used.
  • the system allows for fuel collection from the container or from the line, smooth transformation to gaseous state with simultaneous convenient measurement conditions.
  • an advantage of the system is providing convenient measurement conditions regardless the pressure in the gas pipeline or in the container.

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  • Physics & Mathematics (AREA)
  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Pathology (AREA)
  • Immunology (AREA)
  • General Physics & Mathematics (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Medicinal Chemistry (AREA)
  • Food Science & Technology (AREA)
  • General Chemical & Material Sciences (AREA)
  • Toxicology (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Investigating Or Analysing Materials By Optical Means (AREA)

Claims (4)

  1. Système de mesure de carburants fluides comprenant
    une unité de détection (K1) présentant une chambre de mesure étroite avec au moins deux détecteurs,
    une unité de ramification (T1) destinée à fournir un carburant fluide à l'unité de détection (K1),
    une pompe (P1),
    un manomètre (M1) destiné à mesurer une pression dans la chambre de mesure,
    une unité de commande (C1) destinée à recevoir au niveau d'une entrée un signal en provenance de l'unité de détection (K1),
    dans lequel l'unité de détection (K1) comprend
    un spectromètre à semi-conducteurs sous-térahertz avec une bande passante se trouvant dans une plage de 100 GHz à 1000 GHz et
    un spectromètre térahertz avec une bande passante se trouvant dans une plage de 1 THz à 3 THz,
    dans lequel
    entre l'unité de ramification (T1) et l'unité de détection (K1) il y a une première soupape à pointeau (V1), couplée au manomètre (M1), tandis qu'une sortie de la première soupape à pointeau (V1) est raccordée à une entrée de la chambre de mesure de l'unité de détection (K1) et la sortie de la chambre de mesure est fixée à une seconde soupape apte à être commandée (V2),
    à laquelle la pompe (P1) est raccordée.
  2. Procédé de mesure de carburants fluides au moyen d'au moins deux spectromètres, dans lequel la mesure de carburants fluides est réalisée à l'aide du système tel que défini dans la revendication 1 et la mesure est réalisée par des premières conditions de pression de régulation à l'intérieur de la chambre de l'unité de détection (K1) au moyen de la première soupape à pointeau (V1), de la seconde soupape (V2) et de la pompe (P1), et ensuite en démarrant le spectromètre térahertz et en enregistrant un résultat, et par la suite en réalisant
    une mesure par le détecteur sous-térahertz, avec une bande passante se trouvant dans la plage de 100 GHz à 1000 GHz en tant que dernière mesure.
  3. Procédé selon la revendication 2, dans lequel la mesure est réalisée en ouvrant la première soupape (V1) libérant des vapeurs de carburant, ensuite les mesures sont réalisées avec les spectromètres et un résultat est enregistré, et ensuite la seconde soupape (V2) est ouverte et au moyen de la pompe (P1), des vapeurs de carburant sont évacuées de la chambre de l'unité de détection (K1) par pompage.
  4. Procédé selon la revendication 2, dans lequel en mesurant une pression en continu au moyen du manomètre (M1), une plage d'ouverture de la première soupape (V1) et un fonctionnement de la pompe (P1) et de la seconde soupape (V2) sont régulés afin d'atteindre un état de vide avec un écoulement dynamique dans la chambre de mesure de l'unité de détection.
EP21159799.2A 2020-02-29 2021-02-27 Systeme et procede pour la mesure de carburants fluides Active EP3872477B1 (fr)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
PL433089A PL433089A1 (pl) 2020-02-29 2020-02-29 Układ pomiarowy i pomiaru paliw płynnych za pomocą spektrometru

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EP3872477A1 EP3872477A1 (fr) 2021-09-01
EP3872477C0 EP3872477C0 (fr) 2024-01-31
EP3872477B1 true EP3872477B1 (fr) 2024-01-31

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Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7119697B2 (en) 2004-03-05 2006-10-10 Detector Electronics Corporation Hydrogen fire detection system & method
CN102323235B (zh) 2011-05-27 2013-03-27 中国人民解放军总后勤部油料研究所 一种利用中红外光谱技术测定发动机燃料质量指标的方法
US8748822B1 (en) 2011-06-20 2014-06-10 University Of Massachusetts Chirped-pulse terahertz spectroscopy
EP3001180A1 (fr) 2014-09-29 2016-03-30 Siemens Aktiengesellschaft Procédé et analyseur de gaz pour la mesure de la concentration d'un composant de gaz dans un gaz de mesure

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PL3872477T3 (pl) 2024-04-08
EP3872477C0 (fr) 2024-01-31
PL433089A1 (pl) 2021-08-30
EP3872477A1 (fr) 2021-09-01

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